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# Problem Set I

Chemistry 3100

Winter 2011

## Dr. G. Van Biesen

2.

A sample of runoff water is analyzed for its iron content using two different methods: a direct comparison to a standard iron solution, and a method of standard addition. (a) Direct comparison to a standard iron solution. A 25.0 mL sample of runoff water was acidified with nitric acid and treated with KSCN to form the red complex, FeSCN2+ and diluted to a final volume of 100.0 mL. The absorbance of the solution measured at 480 nm in a 1.00 cm cell was 0.375. A 10.0 mL sample of a reference iron solution containing 5.00 x 10-4 M Fe3+ was treated in the same manner as the sample, including the dilution to a final volume of 100.0 mL. The measured absorbance of this solution was 0.425. Calculate the concentration of iron in mg/L (ppm) in the runoff water. (b) Standard addition. Another 25.0 mL sample of the runoff water is transferred to a 100.0 mL volumetric flask, acidified with nitric acid, and then a 1.00 mL aliquot of 5.00 x 10-3 M Fe3+ is added just before the addition of KSCN to form the same red complex, FeSCN2+. The solution is then brought to volume (100.0 mL). The absorbance of this solution containing the sample and standard was 0.709. Remember that the absorbance for the iron in the runoff sample only was 0.375. Calculate the concentration of iron in ppm in the runoff water using the standard addition data. (c) Which method, direct comparison to a standard solution or standard addition should give the more accurate answer? Explain. Answer: a) 9.86 ppm b) 12.5 ppm

3.

A tissue sample is analyzed for its protein content by the Lowry method. First, a series of standards were prepared containing from 5 to 20 micrograms of a pure protein. After following the Lowry procedure, the absorbance of each standard was measured at 750 nm in a 1.00 cm cell. The data were then subjected to linear least square analysis resulting in the following parameters: m = 0.0162, b = 0.105.

Problem Set I

Chemistry 3100

Winter 2011

## Dr. G. Van Biesen

Next, the tissue sample weighing 2.10 mg was digested to release the protein then diluted to 100.0 mL. A 2.00 mL aliquot of this solution was analyzed by the Lowry procedure in the same manner as the standards resulting in an absorbance of 0.230 in a 1.00 cm cell. Calculate the % protein in the sample. Answer: 18.4 % 4. The molar absorptivity of an aqueous solution of the amino acid tryptophan (204 g/mol) is 5495 at 278 nm. (a) Calculate the expected absorbance at 278 nm of a 4.3 x 10-5M solution of tryptophan if a 1.50 cm cell was employed. (b) What is the molar concentration of a tryptophan solution having an absorbance of 1.16 in a 0.96-cm cell? Answers: a) 0.35 AU b) 2.2 x 10-4 M

5.

The concentration of barbital (a barbiturate) in a blood sample was determined by extraction from 3.00 mL of blood into 15.0 mL of CHCl3 (chloroform). The barbital was then extracted from chloroform with 10.0 mL of 0.045 M NaOH(aq) (pH = 13.00). The absorbance of the solution at 260 nm was measured and found to be 0.115. The pH of a 3.00 mL aliquot of the aqueous solution is then is then adjusted to pH 10* by adding 0.50 mL of 16% of ammonium chloride (NH4Cl). The absorbance of this solution was 0.023. A 30.0 ppm standard barbital solution handled in the same way gave the following results: at pH 13: A = 0.295; at pH = 10, A = 0.002. Calculate the concentration of the barbital in the blood sample in ppm. *At pH =10, barbital does not absorb at 260 nm, any absorption at this pH is due to matrix components. Assume the magnitude of absorbance by the matrix components to be the same at both pH values. Hint : don't forget about dilution for the blank. Answer: 9.0 ppm

6.

A 3.1250 g sample of hair from a person with suspected lead poisoning was analyzed by atomic absorption spectrometry (AAS). The sample was digested to destroy the organic matrix and the resulting solution diluted to 100.0 mL. The absorbance of this solution was 0.250. Next, 0.200 mL of a standard solution containing lead at a concentration of 1.33 x 10-4 mol L-1 is added to 50.0 mL of the sample solution and the absorbance measured giving a value of 0.360. Calculate the lead content of the hair in g Pb per gram (parts-per-million dry weight). Answer: 7.91 ppm

7.

A certain analytical methods is known to give a relative standard deviation of 5 ppt (parts per thousand) or better. A sample is first analyzed three times using this method with the following results: 43.22%, 43.25%, 43.65%. Because the 43.65% result seemed questionable two additional results were obtained as follows: 43.30% and 43.49%. a) What is the relative standard deviation of the first set (n=3) and of the complete set (n=5). 2